Experimental Set-up and Application Research of Solid-State Nuclear Magnetic Resonance Multiple-CP Technique

doi:10.7503/cjcu20200698

Abstract

Abstract:

The quantitative solid-state nuclear magnetic resonance（NMR） multiple-cross polarization（CP） technique attracts enormous interest of the material researchers. With proper setting of experimental parameters， Multiple-CP is capable to determine the molecular chemical structure， multi-phase composition and the component contents of blends. However， the accuracy of the testing results is sensitive to the experimental parameters which are tuned by the system parameters of the measuring samples. To gain the accurate results with high efficiency， it is necessary to reveal the influence behavior of the system parameters on experimental parameters. In this work， L-alanine， L-valine and their mixture were chosen as the model samples. Firstly， system parameters of spin-lattice relaxation time of ¹H（T_1，H）， cross relaxation time（T_CH） and spin?lattice rela-xation time of ¹H in the spin?locking field $(T 1 ρ ? H ?)$ were measured. Meanwhile， the accuracy of Multiple-CP results was evaluated with the variation of three experimental parameters， including relaxation recovery time（t_d）， cross-polarization contact time（t_p）， and cross-polarization times（n）. By comparing the data of different ¹³C groups， it is revealed that the setting of t_p is essential to the result accuracy， which is tuned by T_CH and $? T 1 ρ ? H ?$ of the system. Moreover， the values of the parameter difference between the molecular groups or blended components also affects the Multiple-CP results. Therefore， Multiple-CP is recommended to study the systems with similar T_CH and $? T 1 ρ ? H ?$ values. For the blends or mixtures， the identical unit of each component is suggested chosen for determining the contents.

Key words: Solid-state nuclear magnetic resonance（SSNMR）, Qualification, Multiple-cross polarization, Experimental parameter, Cross-polarization contact time

CLC Number:

O641

TrendMD:

ZHANG Zhilan, WANG Ning, TANG Dandan, SHU Jie, LI Xiaohong. Experimental Set-up and Application Research of Solid-State Nuclear Magnetic Resonance Multiple-CP Technique[J]. Chem. J. Chinese Universities, 2021, 42(3): 784.

Figures/Tables 12

Sample	Carbon	T_CH/ms	T_1,H/ms	$T 1 ρ ? H$ /ms
L?alanine	1	0.170	977.1	1.7
	2	0.042
	3	0.360
L?valine	4	0.160	718.5	2.5
	5	0.036
	6	0.033
	7	0.290
	8	0.150

Sample	Carbon	T_CH/ms	T_1,H/ms	$T 1 ρ ? H$ /ms
L?alanine	1	0.170	977.1	1.7
	2	0.042
	3	0.360
L?valine	4	0.160	718.5	2.5
	5	0.036
	6	0.033
	7	0.290
	8	0.150

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